Preparation of vegetable phosphatides



Patented July 15, 1941 UNITED STATES PATENT OFFICE PREPARATION OF VEGETABLE PHOSPHATIDES Percy L. Julian, Oak Park, and Andrew G. Engstrom, Chicago, 111., assignors to The Glidden Company, Cleveland,' Ohio, a corporation of Ohio No Drawing. Application June 8, 1938 "Serial No. 212,606

' 11 I Claims.

The present invention relates to the recovery of phosphatides from vegetable oil material containing the same. More particularly, the invention relates to the recovery of phosphatides from vegetable oil foots.

It has been proposed in United States Patent No. 2,029,261 to efiect a gravity separation of the phosphatides in soya bean oil from the oil by maintaining hot pressed oil at an elevated temperature for several hours. The sludge which separates out is then centrifuged while hot to remove the remainder of the oil. Heating is essential to this process and, as pointed out in the Schweiger Patent 2,057,695, lecithin is very I dried after separation from the main' body of oil to produce crude lecithin containing about to oil. The crude lecithin is then washed with acetone in which the phosphatides are insoluble, to dissolve the oil, fatty acids and anv This emulsion contains remaining moisture and to remove remaining color resulting in a refined phosphatide low in free fatty acid and of light color. The oil washed out represents a high fatty acid oil and contains considerable color extracted from the crude lecithin.

If the vegetable oils recovered from various materials such as soy bean' oil, corn oil, and others which contain phosphatides, are permitted to stand for any considerable time, the so-called "foots" separate out. These foots are high in phosphatides (25-30%), and contain a large percentage of free fatty acids, coloring matter, and insoluble residue, the remainder being oil. As a considerable amount of such foots are produced in the industry, it is desirable that a satisfactory process for" the recovery of the phos- I phatides in suitable form he provided.

Since the treatment of crude lecithin with acetone, as described above, results in the removal of the fatty oil acids and oil, it is to be expected that a similar treatment of foots would remove the fatty oil acids and oil. It has been found,

however, that when these foots" are washed with acetone, the mass lumps and balls up and the color is not removed. There is no mixing, and as a result, the direct treatment of foots with acetone cannot be resorted to in the production of a satisfactory refined vegetable phosphatide. This lumping and failure to remove color results even when large amounts of acetone are used. Likewise, the addition of bleaching agents to the "foots will not remove the color.-

According to the present invention, a process is provided whereby asatisfactory refined vegetable phosphatide of light color is produced from vegetable oil foots" containing the same.

In carrying out the process, the foots are first dissolved in a substantial quantity of vegetable oil, and any grit or meal present is removed. The solution is then emulsified with water, and preferably subjected to the action of a .bleaching agent, such as hydrogen peroxide, during the emulsification. The use of a bleach is not necessary, but it is desirable for best results, and particularly when the oil is to be re-used. It has also been found that the best bleaching action is obtained if the bleach is present during the emulsiflcation. The .emulsion containing the phosphatides, most of the free fatty acids, some oil and some color is then separated from the I bulk of the oil by centrifuging or other suitable means, and the resulting sludge dried to pro-. duce a crude lecithin. The crude lecithin, containing free fatty acids, some oil and some color can now be purified by washing with acetone.

- The resulting product is a vegetable phosphatide which is a very acceptable product. Most of the fatty oil acids and remaining color have been removed in the acetone washings.

Where bleaching is resorted to, .oil recovered from the centrifuging or other suitable separation may be used over for dissolving more fonts. Since most of the fatty oil acids are thrown down with the phosphatides, there is very little increase in the acid number of the oil, and there is littlechange in color in the oil. It has been found that the oil can be used several times.

The following, are examples of carrying out the invention, but it is to be understood that these examples by no means are exhaustive, and I that the invention is not restricted thereto.

Example I Soy bean expeller oil-foots having the following analysis were treated:

Aoetone Acetone g gggg Free fatty acids in iusolubles extract (oil) Mommas acetone extract Percent Percent Percent Percent 1 Based on original io ts.

200 grams of these foots were dissolved in emulsion can be separated. When using a centrifu'ge, for example, the exact amount may be varied depending upon the setting of the particular centrifuge to give the best separation. The

' amounts necessary to give the best results with any given equipment or method of separation will be readily determined by anyone skilled in the art. 1

The amount of water added may vary, the amount being such that the phosphatides are emulsified in the 011, about 3% by weight of the solution giving an emulsion of the best consist- 1700 cc. of extracted soy bean oil at about 70-80 oil, and separated very nicely. After drying to remove the bulk of the water, the sludge was washed well with acetone to dissolve out the fatty acids, oil, and to remove remaining moisture and most of the remaining color. The residue of 54 grams of light colored refined soya bean lecithin was used to prepare a cocoa butter lecithin by trituration with cocoa butter to give a product of good color and consistency, comparable in every way to cocoa butter lecithin 'prepared from lecithin produced from extracted soy bean oil in the conventional manner. That the free fatty acids were thrown down with the lecithin and washed out with acetone is shown by the presence of 5.54% of free fatty acid in the high acid oil recovered from the acetone wash ings. This high acid oil was of a dark color, and contained a large amount of the color of the crude phosphatide. The oil recovered from the centrifuging was of a light color, with practically no change from the. original oil, and with practically negligible increase in the amount of free fatty acids.

Example II 450 pounds of the "foots" from expeller soy bean oil were dissolved in approximately 500 gallons of lecithin-free extracted soy bean oil. After the removal of grit and meal, the solution was emulsifledwith 16 gallons of water and 2 gallons of a solution of hydrogen peroxide. The emulsion was then centrifuged, the sludge dried and washed with acetone as above. The refined. soy bean lecithin produced was of good color and comparable in all respects with that produced by the regular process from extracted oil.

The above examplesare to be considered as illustrative only, as'various changes and modifications may be made therein without departing from the spirit of the invention. It is not necessary that soy bean oil be used, as any other suitable oil can be used. Also. the oil need not be freed' from its phosphatide content before use. Thus, by usingoil containing its natural phosphatidecontent, the capacity of a given producing unit can be doubled.

The amount of oil used may vary over rather wide limits. The amount should be sufiicient to dissolve the phosphatide, oil, acids and other solubles and to give a solution from which the lecithinency for handling and centrifuging. The process may be carried out by using between 2.5 and 6% of water, or more or less, although it is preferred to operate within the range just specified. Any other suitable bleaching agent can be used, such assodium peroxide, benzoyl peroxide, etc., the

amount used being more or less depending upon the degree of bleaching desired. In place of acetone, any volatile solvent which is a solvent for the fatty acids and oil and which is a non-solvent for the phosphatides, such as acetic esters (methyl acetate. ethyl acetate), may be used.

Having described our invention, what is claimed as new and desired to secure by Letters Patent of the United States is:

1. The process of recovering vegetable phos phatides from vegetable oil foots containing phosphatides which comprises dissolving the "foots" in a vegetable oil, emulsifying the phosphatides in the solution with water, separating the emulsion from the oil, and recovering the phosphatides from the emulsion.

2. The process of recovering vegetable phosphatides which comprises dissolving vegetable oil foots containing phosphatides in a vegetable oil, emulsifying the solution with water, separating the emulsion from the oil, removing the water from the emulsion and extracting the residue with acetone.

3. In the process of preparing vegetable phosphatide from vegetable oil "foots containing the same, the steps comprising dissolving the foots" in a vegetable oil, then emulsifying the solution with water in the presence of a bleachdue with a solvent for oil and free fatty acids" which is a, non-solvent for the phosphatides.

5. The process which comprises dissolving vegetable oil foots" containing phosphatides in a vegetable oil containing'phosphatides, emulsifying'the phosphatides in the solution with water, separating the emulsion from the oil and rccovering the phosphatides from the emulsion.

6. The process of treating soy bean oil foots" to. recover the phosphatides therefrom which comprises dissolving the "foots" in soy bean oil,

, emulsifying the phosphatides in the solution with to recover the phosphatides therefrom, which comprises dissolving the "foots" in soy bean oil,

8. The process of claim 6 in which the soy bean oil used contains phosphatides.

9. The process of treating vegetable oil roots containing phosphatides and a large amount of coloring matter, which comprises dissolving the feats in a vegetable oil, emulsifying the phosphatides with water containing a bleaching agent in solution, separating the emulsion from the bulk of the oil, drying the emulsion, and wash-' ing the crude phosphatides so produced with a solvent for the oil and free fatty acid present and which is a non-solvent for the phosphatides, whereby there is produced a refined phosphatide or light color.

10. The process of preparing refined vegetable phosphatides which comprises dissolving vegetable oilroots containing phosphatides in a vegetable oil, emulsifying the phosphatides in the solution with water in the presence of a bleaching agent, separating the emulsion from the bulk of the oil to produce alight colored oil portion and an emulsified fraction containing phosphatides, water, tree fatty acids, some oil and the remaining color, drying the emulsion to produce a crude phosphatide, washing the crude phos phatide with a solvent for the'oil and free fatty acids which is a non-solvent for the phosphatides whereby a purified phosphatide is produced, dissolving more "Ioots in the light colored oil fraction, and repeating the process.

11. In the process of recovering purified phosphatides from vegetable oil foots containing the same, the step consisting in dissolving the facts in a vegetable oil which is a solvent for the phosphatides, oil, fatty acids, coloring matter, and other soluble ingredients of the foots, prior to any bleaching extraction or other purification steps.

PERCY L. JULIAN. ANDREW G. ENGSTROM. 

